Strontium cobaltite oxygen sponge catalyst and methods of use
09550166 ยท 2017-01-24
Assignee
Inventors
- Ho Nyung Lee (Oak Ridge, TN)
- Hyoungjeen Jeen (Knoxville, TN, US)
- Woo Seok Choi (Gyeonggido, KR)
- Michael Biegalski (Oak Ridge, TN, US)
- Chad M. Folkman (San Jose, CA, US)
- I-Cheng Tung (Chicago, IL, US)
- Dillon D. Fong (Elmhurst, IL, US)
- John W. Freeland (Oak Park, IL, US)
- Dongwon Shin (Knoxville, TN, US)
- Hiromichi Ohta (Sapporo, JP)
- Matthew F. Chisholm (Oak Ridge, TN, US)
Cpc classification
B01J35/33
PERFORMING OPERATIONS; TRANSPORTING
B01J23/78
PERFORMING OPERATIONS; TRANSPORTING
C01G51/66
CHEMISTRY; METALLURGY
B01J20/04
PERFORMING OPERATIONS; TRANSPORTING
C01P2002/72
CHEMISTRY; METALLURGY
B01J37/349
PERFORMING OPERATIONS; TRANSPORTING
B01J23/002
PERFORMING OPERATIONS; TRANSPORTING
C01P2002/77
CHEMISTRY; METALLURGY
International classification
B01J23/58
PERFORMING OPERATIONS; TRANSPORTING
B01J23/78
PERFORMING OPERATIONS; TRANSPORTING
B01J23/847
PERFORMING OPERATIONS; TRANSPORTING
B01J20/04
PERFORMING OPERATIONS; TRANSPORTING
Abstract
Rapid, reversible redox activity may be accomplished at significantly reduced temperatures, as low as about 200 C., from epitaxially stabilized, oxygen vacancy ordered SrCoO.sub.2.5 and thermodynamically unfavorable perovskite SrCoO.sub.3-. The fast, low temperature redox activity in SrCoO.sub.3- may be attributed to a small Gibbs free energy difference between the two topotactic phases. Epitaxially stabilized thin films of strontium cobaltite provide a catalyst adapted to rapidly transition between oxidation states at substantially low temperatures. Methods of transitioning a strontium cobaltite catalyst from a first oxidation state to a second oxidation state are described.
Claims
1. A catalyst comprising epitaxially stabilized strontium cobaltite having a first oxidation state that reversibly transitions to a second oxidation state at a temperature of between about 200 C. and about 340 C., wherein: one of said first and second oxidation states is defined as SrCoO.sub.3-; is less than or equal to 0.1; and the other of said first and second oxidation states is defined as SrCoO.sub.2.5, wherein the strontium cobaltite is stabilized on a substrate selected from the group consistin of: perovskite (ABO.sub.3), SrTiO.sub.3, and (LaAlO.sub.3).sub.0.3(Sr.sub.2AlTaO.sub.6).sub.0.7; and wherein A is selected from the group consisting of an alkaline metal and an alkaline earth element, and B is a transitional metal.
2. The catalyst of claim 1, wherein the catalyst in said first oxidation state is ferromagnetic and electro-conductive and the catalyst in said second oxidation state is antiferromagnetic and electro-insulating.
3. The catalyst of claim 1, wherein said transition from said first oxidation state to said second oxidation state occurs in less than about 1 minute.
4. The catalyst of claim 1, wherein said transition from said first oxidation state to said second oxidation state occurs at a temperature of between about 210 C. and about 320 C.
5. The catalyst of claim 1, wherein said transition from said first oxidation state to said second oxidation state is rapidly reversible at a temperature greater than or equal to 200 C.
6. The catalyst of claim 1, wherein said transition from said first oxidation state to said second oxidation state is a reduction process, said first oxidation state is strontium cobaltite in a perovskite phase, and said second oxidation state is strontium cobaltite in a brownmillerite phase.
7. The catalyst of claim 6, wherein said reduction process is completed in less than about 1 minute and at a temperature of between about 210 C. and about 320 C.
8. The catalyst of claim 6, wherein said transition from said first oxidation state to said second oxidation state is a reversible process, said reversible process is an oxidation process, and said brownmillerite phase of said strontium cobaltite is oxidized to said perovskite phase of said strontium cobaltite.
9. The catalyst of claim 8, wherein said oxidation process is completed in less than about 1 minute and at a temperature of between about 210 C. and about 320 C.
10. The catalyst of claim 8, wherein said perovskite phase of said strontium cobaltite is SrCoO.sub.3-.
11. An article comprising a thin film having the catalyst of claim 1.
12. The article of claim 11, wherein the article is an electromechanical device.
13. The article of claim 12, wherein said electromechanical device is selected from the group consisting of: a fuel cell, an electrolyzer, a battery, a sensor, and a catalytic converter.
14. An epitaxially stabilized thin film of strontium cobaltite having a first oxidation state that reversibly transitions to a second oxidation state at a temperature of between about 200 C. and about 340 C., wherein: one of said first and second oxidation states is defined as SrCoO.sub.3-; is less than or equal to 0.1; and the other of said first and second oxidation states is defined as SrCoO.sub.2.5, wherein the strontium cobaltite is stabilized on a substrate selected from the group consisting of: pervoskite (ABO.sub.3), SrTiO.sub.3, and (LaAlO.sub.3).sub.0.3(Sr.sub.2AlTaO.sub.6).sub.0.7; and wherein A is selected from the group consisting of an alkaline metal and an alkaline earth element, and B is a transitional metal.
15. A method of transitioning the catalyst of claim 1 comprising epitaxially stabilized strontium cobaltite between a first oxidation state and a second oxidation state, the method comprising the steps of: providing a substrate supporting at least a thin layer of said catalyst in said first oxidation state; elevating a temperature of said catalyst in said first oxidation state; and providing a vacuum atmosphere to said catalyst in said first oxidation state; wherein the temperature is elevated to within a range of about 210 C. to about 320 C. for a period of time to effect transition of said catalyst from said first oxidation state to said second oxidation state.
16. The method of claim 15, wherein the period of time is less than about 1 minute.
17. The method of claim 15, wherein said catalyst in said first oxidation state is in a perovskite phase and said catalyst in said second oxidation state is in a brownmillerite phase.
18. The method of claim 15, wherein the period of time is further defined as a first period of time and further comprising the steps of: elevating a temperature of said catalyst in said second oxidation state; and providing oxygen to said catalyst in said second oxidation state for a second period of time; wherein the second period of time is sufficient to effect transition of said catalyst from said second oxidation state back to said first oxidation state.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
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(21) Before the embodiments of the invention are explained in detail, it is to be understood that the invention is not limited to the details of operation or to the details of construction and the arrangement of the components set forth in the following description or illustrated in the drawings. The invention may be implemented in various other embodiments and is capable of being practiced or being carried out in alternative ways not expressly disclosed herein. Also, it is to be understood that the phraseology and terminology used herein are for the purpose of description and should not be regarded as limiting. The use of including and comprising and variations thereof is meant to encompass the items listed thereafter and equivalents thereof as well as additional items and equivalents thereof. Further, enumeration may be used in the description of various embodiments. Unless otherwise expressly stated, the use of enumeration should not be construed as limiting the invention to any specific order or number of components. Nor should the use of enumeration be construed as excluding from the scope of the invention any additional steps or components that might be combined with or into the enumerated steps or components.
DESCRIPTION OF THE CURRENT EMBODIMENT
(22) A catalyst in accordance with an embodiment of the invention is shown in
(23) Directional terms, such as vertical, horizontal, top, bottom, upper, lower, inner, inwardly, outer and outwardly, are used to assist in describing the invention based on the orientation of the embodiments shown in the illustrations. The use of directional terms should not be interpreted to limit the invention to any specific orientation(s).
(24) Referring to
(25) Epitaxial SrCoO.sub.2.5 and SrCoO.sub.3- thin films (40-60 nm in thickness) were grown on (001) STO and (001) LSAT substrates by pulsed laser epitaxy (KrF, =248 nm). The films were grown at 750 C. in 0.013 mbar of O.sub.2 for the SrCoO.sub.2.5 and 0.267 mbar of O.sub.2+O.sub.3 (5%) for the SrCoO.sub.3-. The laser fluence was fixed at 1.7 J/cm.sup.2. The sample structure and crystallinity were characterized by high-resolution four-circle XRD (XPert, Panalytical Inc.). The Z-contrast images were obtained using a Nion Ultra STEM 200 operated at 200 keV.
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(27) Confirmation of the two chemically distinct phases was provided by observing the details of the cobalt valence state of epitaxial SrCoO.sub.2.5 and SrCoO.sub.3- thin films by polarized x-ray absorption spectroscopy (XAS). This technique provides information on the oxidation state of cobalt which plays a deterministic role in the magnetic, electronic and catalytic properties of the materials. Oxygen stoichiometry in the SrCoO.sub.2.5 and SrCoO.sub.3- thin films were qualitatively characterized by monitoring the oxygen K-edge peaks as shown in
(28) The distinct chemical valence difference between the SrCoO.sub.2.5 and SrCoO.sub.3- phases produced distinct magnetic and electric properties. Element-resolved measurements of the net magnetic moment using x-ray magnetic circular dichroism (XMCD) showed a large ferromagnetic signal in the SrCoO.sub.3- film, see
(29) There are also different electron transport properties between the two phases. Referring to
(30) The valence (or oxidation) state and magnetism in SCO was elucidated by XAS and XMCD at beamline 4-ID-C of the Advanced Photon Source, Argonne National Laboratory. Magnetic property was characterized with a 7 T Superconducting Quantum Interference Device (SQUID) magnetometer (Quantum Design). Temperature dependent DC transport measurements with van der Pauw geometry were performed with a 14 T Physical Property Measurement System (PPMS) (Quantum Design). The thermopower values were also measured by a conventional steady state method using two Peltier devices under the thin films to give a temperature difference (V10K). Unlike the other measurements to eliminate the different substrate contributions during the thermopower measurements, both SrCoO.sub.3- and SrCoO.sub.2.5 films used were grown on (001) STO substrates.
(31) Reversible redox reactions were monitored for a SrCoO.sub.3- to SrCoO.sub.2.5 conversion and SrCoO.sub.2.5 to SrCoO.sub.3- conversion. These reactions were observed by XRD, in which several parameters may be controlled, such as but not limited to, gas type, flow rate and pressure. During the SrCoO.sub.3- to SrCoO.sub.2.5 conversion a high-resolution four-circle XRD (XPert, Panalytical Inc.) with a domed hot stage (DHS 900, Anton Paar) was used. The inside of the dome was evacuated with a mechanical pump to a base pressure of 0.0013 mbar. For the SrCoO.sub.2.5 to SrCoO.sub.3- conversion, a power XRD with reactor chamber (XRK 900, Anton Paar) was used to pressurize the inside of the heating chamber to about 5 bar of O.sub.2. The temperature ramping rate was between about 30-60 C. per minute with an average scan time of about 2 to 2.5 minutes. To demonstrate the phase reversal processes, real-time readings of temperature dependent XRD -2 scans with epitaxial films on LSAT in vacuum and with an oxygen atmosphere were recorded.
(32) The ability to control the oxygen content in a material is significant for both physics and for technological application of multivalent oxides. Reversible oxidation-reduction (redox) reactions were directly observed between the epitaxially stabilized perovskite and brownmillerite phases of strontium cobaltite without destruction or degradation of the parent material. Results of direct probing of reversible redox activity are shown in
(33) For the oxidation process (SrCoO.sub.2.5 to SrCoO.sub.3-), complete oxidation may be achieved at about 350 C. in 5 bar of O.sub.2, as shown in
(34) The energy barrier for the phase transition of
(35) Thermodynamic descriptions for SrCoO.sub.2.5 and SrCoO.sub.3- were taken from the thermodynamic modeling of strontium cobaltite for which model parameters were critically and self-consistently evaluated to reproduce both phase equilibrium and thermochemistry data in their bulk form. All the equilibrium phases in the thermodynamic modeling of strontium cobaltite other than SrCoO.sub.2.5 and SrCoO.sub.3- were suspended in the thermodynamic calculation to compute only the energy difference between SrCoO.sub.2.5 and SrCoO.sub.3-. Thermo-Calc software was used to minimize the individual Gibbs energies of the strontium cobaltite phases at given temperatures and oxygen contents. Thermodynamic descriptions for SrCoO.sub.2.5 and SrCoO.sub.3- were obtained from the 2010 Ph.D. thesis of J.E. Saal at the University of Pennsylvania. SrCoO.sub.2.5 and SrMnO.sub.2.5 were modeled as stoichiometric, while the perovskite phases were modeled as solution phases. The latter's designated oxygen sub-lattices allowed for mixing between oxygen and vacancy to achieve hypo-stoichiometry.
(36) Fast, reversible redox activity is useful to provide catalytic activity at relatively low temperatures. Carbon monoxide oxidation probe reactions were conducted to elucidate the use of strontium cobaltite as a heterogeneous catalyst. Due to the extremely small surface areas of the epitaxial films, a custom designed micro-reactor was used with inlet gas streams of CO (0.1 mbar) and O.sub.2 (0.1 mbar). The effluent gas mixture was analyzed in-line with a gas-chromatograph and mass spectroscopy detector. For this reaction, the oxygen activity in the reactor was low; thus the epitaxial SrCoO.sub.3- film was unstable and the epitaxial SrCoO.sub.2.5 film on LSAT was chosen for the catalytic study. Catalytic activity can be connected to both the consumption of CO and the production of CO.sub.2. The conversion of the inlet CO gas is shown in
(37) Gas-phase catalysis measurements were made with a custom micro-reactor with a volume <50 mL. A high level of reactor cleanliness was achieved by limiting material within the reactor to fused quartz, stainless steel and fluoropolymer seals. Heating was conducted by passing light from a halogen bulb through a fused quartz platform to the backside of the sample. The inlet gas streams consisted of 300 ppm CO and 300 ppm O.sub.2, both mixed with a helium balance (resulting in a partial pressure of 0.1 mbar for each gas), and a throughput of 5 SCCM. The temperature was programmed at 30 C. intervals each held for 16 minutes. At each interval the initial 10 minutes were reserved to allow the system to reach steady state conditions. Afterwards, a 20 l aliquot of the gas stream was injected into the gas chromatograph / mass spectrometer (PERKINS ELMER). A carbon packed capillary column was used to separate the CO and residual N.sub.2 in the gas sample. The total ion chromatogram was mass separated to isolate peaks from CO and CO.sub.2 and then integrated. The concentration was determined with the integrated values and calibrated values from known gas mixtures. Detection limits for the CO conversion were set by the surfaces within the reactor, as determined by running the temperature program without a sample loaded and measuring the CO levels. In contrast, the detection limit for CO.sub.2 was set by the sensitivity of the mass spectrometer (4ppb). The reproducibility of the conversion trends was substantiated with measurement of an additional SrCoO.sub.2.5 epitaxial thin film.
(38) The above description is that of current embodiments of the invention. Various alterations and changes can be made without departing from the spirit and broader aspects of the invention as defined in the appended claims, which are to be interpreted in accordance with the principles of patent law including the doctrine of equivalents. This disclosure is presented for illustrative purposes and should not be interpreted as an exhaustive description of all embodiments of the invention or to limit the scope of the claims to the specific elements illustrated or described in connection with these embodiments. For example, and without limitation, any individual element(s) of the described invention may be replaced by alternative elements that provide substantially similar functionality or otherwise provide adequate operation. This includes, for example, presently known alternative elements, such as those that might be currently known to one skilled in the art, and alternative elements that may be developed in the future, such as those that one skilled in the art might, upon development, recognize as an alternative. Further, the disclosed embodiments include a plurality of features that are described in concert and that might cooperatively provide a collection of benefits. The present invention is not limited to only those embodiments that include all of these features or that provide all of the stated benefits, except to the extent otherwise expressly set forth in the issued claims. Any reference to claim elements in the singular, for example, using the articles a, an, the or said, is not to be construed as limiting the element to the singular.